反应详情

To a solution of ethyl 2-oxopiperidine-4-carboxylate (10.76 g, 62.85 mmol) in toluene (120 mL) was added the Lawesson's reagent (25.42 g, 62.85 mmol) under a nitrogen atmosphere. The mixture was heated to reflux for 2 h. Removed the solvent under reduced pressure and the residue was purified by silica gel column chromatography (DCM/EA=20/1) to afford ethyl 2-thioxopiperidine-4-carboxylate (5.8 g, yield 49.3%).

1. temperatureThe mixture was heated
2. temperatureto reflux for 2 h
3. customRemoved the solvent under reduced pressure
4. customthe residue was purified by silica gel column chromatography (DCM/EA=20/1)